Validation services for analytical methods in a laboratory

Validation of an analytical method is an essential step in demonstrating that the method is fit for its intended purpose. It confirms that the method produces reliable and reproducible results that meet scientific and regulatory expectations. Organisations such as ICH, the FDA and ISO 17025 define the parameters to be verified: accuracy, precision (repeatability and reproducibility), specificity, limit of detection (LOD), limit of quantification (LOQ), linearity, measurement range and robustness. 

Used for regulatory purposes (which are themselves linked to product quality and safety considerations), it requires a preliminary framework to define the parameters to be met, such as sample preparation, the technique to be used, its parameters, its environment, the expected results, acceptable uncertainty, timelines, etc. These criteria must be set out and signed in a study protocol before validation begins.

When choosing a method validation laboratory, several criteria should be considered. First and foremost, it is essential to assess the laboratory’s skills and expertise in the specific field of the method to be validated.

You can therefore review the laboratory’s references, previous experience and the technical skills of its staff. 

It is also important to verify the laboratory’s certifications and accreditations. Accreditations issued by recognised organisations such as ISO demonstrate the laboratory’s competence and compliance with quality and reliability standards. 

Finally, it is recommended to choose a method validation laboratory equipped with state-of-the-art infrastructure and equipment. 

By taking these various factors into account, you can choose a competent and reliable laboratory to carry out your method validation. With a team of experts and more than 2,000 m² of analytical facilities, FILAB offers method validation services, as well as research and development support.

During a laboratory method validation, our experts seek to verify whether the analytical method is suitable for the analyte or compound being measured, according to various criteria:

• The method is sufficiently sensitive and capable of detecting the lowest levels,
• The method is specific, measuring the desired analyte without interference from other compounds present in the sample.
• The method is precise and reproducible, making it possible to produce consistent results when repeated.
• The method is robust, making it possible to produce reliable results despite variations in the analysis conditions. 
• The method used is appropriate in terms of limits of detection and quantification, making it possible to detect and accurately measure the lowest levels of the analyte. 
• The method is compliant with regulatory requirements and industry standards.
• The method incorporates quality control procedures to ensure the validity of the results obtained. 
• The method details the protocols, including the acceptance criteria for each parameter evaluated.

These questions help assess all relevant aspects of an analytical method to ensure its reliability and suitability for laboratory use.

Analytical methods are the techniques used to identify, quantify or characterise a compound or matrix. They can be divided into broad families: chromatographic methods (HPLC, GC, IC), spectroscopic methods (UV-Vis, IR, NMR, ICP-OES, ICP-MS), electrochemical methods, titrimetric or gravimetric methods, and hyphenated techniques such as LC-MS or GC-MS. Each method is based on a physical or chemical principle and must be validated in the context of its application. 

No. Analytical validation criteria depend both on the nature of the method and its purpose. For example, an HPLC chromatographic method used to quantify an active ingredient in a pharmaceutical formulation must meet strict criteria for linearity, accuracy, precision and quantification limits, in order to ensure assay accuracy. Conversely, infrared spectroscopy (IR) used to identify an impurity will place greater emphasis on specificity and robustness, since the primary objective is the qualitative identification of a compound rather than its precise quantification.

Test method validation consists of demonstrating that the test method used in a laboratory produces reliable results that are fit for the purpose of the test. It applies in particular to laboratories accredited to ISO 17025, where each test method must be validated or verified before use. Test method validation involves evaluating the performance of the method as a whole, taking into account the sample, matrix and analytical context. It ensures that the results obtained meet the expected quality criteria, both technically and from a regulatory standpoint.

Analytical procedure validation focuses on the operational application of a method within a laboratory. An analytical procedure is a detailed protocol describing all the steps required to implement a method: sample preparation, operating conditions, instrumental parameters, data processing and acceptance criteria. Analytical procedure validation therefore consists of demonstrating that, under the specific conditions defined by the laboratory, the procedure produces compliant and robust results. It is essential for ensuring day-to-day reliability, reducing the risk of error and guaranteeing regulatory compliance.

Analytical validation is the generic term encompassing the entire validation process. 

Validation of an analysis method or analytical method focuses on the scientific technique itself (e.g. chromatography, spectroscopy). 

Test method validation is often used in accredited laboratories and refers to the validation of tests applied to real samples. 

Finally, analytical procedure validation is more operational and concerns the detailed protocol implemented in a specific laboratory. 

A validated analytical method needs to be maintained! It is recommended that every validated method be monitored to ensure that it remains suitable for its intended use throughout its lifecycle. To this end, the implementation of control charts makes it possible to monitor the reliability of the method used routinely.

Furthermore, in the event of a change, it will be necessary to assess whether partial or full revalidation is required, depending on the circumstances. Among the non-exhaustive list of changes that lead to analytical method revalidation, ICH Q2(R1) cites changes to the composition of the finished product, raw materials or analytical procedures (criteria).